My PhD dissertation - Institut Fresnel

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1 H NMR: δ = 1.7 (m, 6 H), 1.5 (m, 2 H), 1.4 (m, 2 H), 1.17 (dt, J = 15.6, 7.7 Hz,
6 H), 0.94 (t, J = 7.2 Hz, 3 H) ppm.
13 C NMR: δ = 26.2 (d, J = 65 Hz), 24.2 (d, J = 14 Hz), 23.5 (d, J = 4 Hz), 19.8 (d,
J = 66 Hz), 13.6, 5.7 (d, J = 5 Hz) ppm.
31 P NMR: δ = 58.1 ppm.
Butyldimethylposphine oxide (27f): A 30% aqueous hydrogen peroxide solution (3.5 mL,
29 mmol) was added dropwise to a solution of butyldimethylphosphine (26i; 2.3 g, 19 mmol)
in diethyl ether (38 mL) at 0 °C. After the exothermic reaction has ceased, phases were
separated and the organic layers was washed with a saturated sodium sulfite solution (10 mL)
and dried with sodium sulfate. Removal of the solvent and distillation of the residue afforded
a colorless liquid; b.p. 81 - 82 °C/0.35 Torr (ref. [38] b.p. 70 - 73 °C/0.25 Torr; yield: 2.18 g
(84%).
1 H NMR: δ = 1.7 (m, 2 H), 1.6 (m, 2 H), 1.48 (d, J = 12.3 Hz, 6 H), 1.45
(symm. m, 2 H), 0.95 (t, J = 7.2 Hz, 3 H) ppm.
13 C NMR: δ = 31.5 (d, J = 69 Hz), 24.1 (d, J = 20 Hz), 24.0, 16.1 (d, J = 68 Hz),
13.6 ppm.
31 P NMR: δ = 45.6 ppm.
Butyldicyclohexylphosphine oxide (27g): Analogously prepared from
butyldicyclohexylphosphine (26j; 2.7 g, 15 mmol) and 30% hydrogen peroxide solution
(5 mL); white needles after sublimation; m.p. 57 - 59 °C; yield: 3.77 g (93%).
1 H NMR: δ = 2.0 (m, 3 H), 1.8 (m, 6 H), 1.7 (m, 3 H), 1.6 (m, 4 H), 1.4 (m, 6 H),
1.2 (m, 6 H), 0.93 (t, J = 7.3 Hz, 3 H) ppm.
13 C NMR: δ = 36.3 (d, J = 64 Hz), 26.6 (d, J = 3 Hz), 26.6 (d, J = 3 Hz), 26.0 (d, J = 1
Hz), 26.0 (d, J = 2 Hz), 25.7 (d, J = 3 Hz), 24.7 (d, J = 13 Hz), 24.1 (d, J = 4 Hz), 23.6
(d, J = 61 Hz), 13.7 ppm.